CN104945652A - Nylon with highly hard and abrasion resistant surface and preparation method thereof - Google Patents
Nylon with highly hard and abrasion resistant surface and preparation method thereof Download PDFInfo
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- CN104945652A CN104945652A CN201510437017.8A CN201510437017A CN104945652A CN 104945652 A CN104945652 A CN 104945652A CN 201510437017 A CN201510437017 A CN 201510437017A CN 104945652 A CN104945652 A CN 104945652A
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Abstract
The invention discloses nylon with a highly hard and abrasion resistant surface and a preparation method thereof. The nylon with the highly hard and abrasion resistant surface adopts the technical scheme as follows: a gradient hardening abrasion-resistant layer is arranged on the nylon surface; the gradient hardening abrasion-resistant layer comprises Si-C reticular cross-linking layer and an inorganic carbonized layer from outside to inside; the depth of the gradient hardening abrasion-resistant layer is 1-6 microns; the percentage content of the carbon atoms in the inorganic carbonized layer is not lower than 95%; the depth of the inorganic carbonized layer is 0.5-5 microns. According to the preparation method, nylon is fixed on the target table of an ion implanter, firstly argon plasma is adopted to activate the material surface in a vacuum condition to form the inorganic carbonized layer, and silicon plasma or silicon/ nitrogen plasma is injected to form an inorganic compound hardening abrasion-resistant layer; the method is easy to operate, and has no effect on the physical-chemical structure of the nylon body; the obtained nylon after treatment is stable in surface structure, high in surface rigidity and good in abrasion resistance, and can be widely used in structural load-bearing components.
Description
Technical field
The present invention relates to engineering plastic modification technical field.More specifically, the preparation method of the high hard wear resistant nylon in a kind of surface is related to.
Background technology
Nylon (Nylon) has another name called polymeric amide, developed by the R&D team under E.I.Du Pont Company's Tomas Carothers thirties in 20th century (Carothers) and leader thereof, refering in particular to Nylon66 at first, is the fiber of the first synthetic in the world.Subsequently, along with updating of technique for synthesizing nylon, the commercialization of nylon expands to multiple trades mark such as nylon 6, nylon 11, nylon 12 from initial nylon66 fiber, Application Areas also from initial textile fiber extension to structural engineering plastics field, has now become one of most widely used engineering plastics.But, owing to there being the amido linkage of strong polarity in nylon molecules chain, water-absorbent is strong, the dimensional stability of finished product product is poor, and the hydrogen bond in nylon molecules interchain and molecular chain makes the interaction between molecular chain very strong, higher than common plastics surface energy, when contacting with some materials, bonding strength is strong, frictional coefficient is large, causes wear resisting property not enough, limits its application in bearing, gear, liner, tightness system and joint prosthesis equivalent-load field.
In order to improve the wear resisting property on nylon surface, current mainly through increasing matrix rigid, adding wear resistance filler and realize the method that article surface directly carries out modification.In nylon, add fortifying fibre such as glass fibre, carbon fiber, aramid fiber etc. significantly can increase the rigidity of nylon composite materials, improve the surface hardness of material, but limited to the lifting of composite-material abrasive; And the filler adding wear resistance such as molybdenumdisulphide, carbon black, polytetrafluoroethylene powder, silicone powder etc. can improve the wear resisting property of nylon composite materials preferably, but the addition of wear resistant filler is larger.No matter be the melt fluidity that fortifying fibre or wear resistant filler all can reduce matrix material, the processability of material declines, and is unfavorable for preparing baroque product.In addition, for the directly modification of nylon products surface, general employing chemical vapour deposition or Magnetron Sputtered DLC coating (DLC) or other wear-resistant coating realize, due to diamond-like coating (DLC) or other wear-resistant coating rigidity stronger, and nylon substrates rigidity of material is more weak, cause bonding interface layer internal stress comparatively large, the bonding force of coating and nylon substrates is poor, and life-time service coating is easily peeled off from substrate and causes material failure.
In prior art, for surperficial Hardening and the wear-resisting modification of nylon products, the main method adopting blending and modifying to add fortifying fibre and wear resistant filler realizes.But generally need add fortifying fibre and the wear resistant filler of high level, the filler of high-content is unfavorable for that the injection molding of nylon is shaping, is difficult to prepare baroque product.Also adopt in addition and carry out direct modification of nylon and to realize Hardening wear-resisting in the vapour deposition of nylon surface chemistry or Magnetron Sputtered DLC coating (DLC) or other wear-resistant coating.Because diamond-like coating (DLC) or other wear-resistant coating rigidity are comparatively strong, and nylon substrates rigidity of material is more weak, causes bonding interface layer internal stress comparatively large, and the bonding force of coating and nylon substrates is poor, and life-time service coating is easily peeled off from substrate.The present invention is directed to the deficiencies in the prior art, the method that using plasma injects, gradient Hardening wearing layer is built at nylon surface in situ, modified layer and substrate nylon combine together, there is not the situation that modified layer is peeled off from nylon substrates, belong to goods post-processing technology, do not affect Drawing abillity, baroque product can be processed, overcome deficiency of the prior art well, there is boundless application prospect.
Beneficial effect of the present invention is as follows:
1) the present invention's technical scheme used belongs to the aftertreatment surface modification of finished product product, and modified layer is shallow, does not affect the bulk properties of product, as physical and chemical performances such as tensile strength, shock strength, flexural strength and heat-drawn wires.
2) the present invention adopts ion implantation method to prepare Hardening wearing layer at nylon surface in situ, compared with the surface deposition class method of modifying such as magnetron sputtering, modified layer and substrate caking power strong, modified layer difficult drop-off.
3) the high hard wear resistant nylon in prepared surface of the present invention can be used for wear-resistant gear equivalent-load structural element.
Summary of the invention
One object of the present invention is to provide a kind of surface high hard wear resistant nylon.This modification of nylon modified layer is shallow, does not affect the bulk properties of product, as physical and chemical performances such as tensile strength, shock strength, flexural strength and heat-drawn wires, can be widely used in structural load bearing component.
Another object of the present invention is the preparation method providing the high hard wear resistant nylon in a kind of surface.The method can not have an impact to the performance of nylon and composite body thereof, does not affect Drawing abillity; The nylon surface tissue obtained after process is stablized, and surface hardness is high, and wear resisting property is good.
For reaching above-mentioned first object, the present invention adopts following technical proposals:
The high hard wear resistant nylon in a kind of surface, is characterized in that: described nylon surface has gradient Hardening wearing layer; Described gradient Hardening wearing layer is the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad; The degree of depth of described gradient Hardening wearing layer is 1 ~ 6um; Carbon atom percentage composition in described inorganic carbide layer is not less than 95%; The degree of depth of described inorganic carbide layer is 0.5 ~ 5um.
Preferably, institute's gradient Hardening wearing layer is the N-Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.
Preferably, described nylon is selected from one or more in the matrix material of nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and various nylon based.
For reaching above-mentioned second object, the present invention adopts following technical proposals:
The preparation method of the high hard wear resistant nylon in a kind of surface as above, adopts ion implanter to build the inorganic Hardening wearing layer of gradient at nylon surface in situ.
Preferably, described preparation method comprises the steps:
1) nylon products ethanol and deionized water are cleaned up respectively rear naturally dry for subsequent use;
2) by step 1) in the nylon that obtains insert on ion implanter target platform, with 4 × 10
15~ 5 × 10
17ion/cm
2dosage inject argon plasma, activated nylon molecular chain, form inorganic carbide layer on nylon surface; In whole injection process maintenance injection chamber, pressure is not higher than 3 × 10
-2pa, target platform temperature is 80 ~ 110 DEG C; After injection completes in chamber pressure not higher than 3 × 10
-210 ~ 30min is kept under Pa;
3) in ion implanter by step 2) in treated nylon in cavity pressure not higher than 5 × 10
-3under Pa, take HIGH-PURITY SILICON as negative electrode, with 6 × 10
15~ 6 × 10
17ion/cm
2dosage inject silicon plasma body, thus the high hard wear resistant nylon in obtained surface.
Preferably, step 1) in, described nylon be selected from the matrix material of nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and various nylon based one or more.
Preferably, step 2) in, the carbon atom percentage composition in described inorganic carbide layer is not less than 95%; The degree of depth of described inorganic carbide layer is 0.5 ~ 5um.
Preferably, step 3) in, the surface in situ of the high hard wear resistant nylon in obtained surface forms the gradient Hardening wearing layer of the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad; The degree of depth of described gradient Hardening wearing layer is 1 ~ 6um.
Preferably, step 3) in, after silicon plasma body injects, also comprise and pass into High Purity Nitrogen again, in cavity, pressure is not higher than 3 × 10
-2under Pa, by 2 × 10
15~ 6 × 10
17ion/cm
2the nitrogen plasma of dosage injects nylon surface, thus the high hard wear resistant nylon in obtained surface; The surface in situ of the high hard wear resistant nylon in described surface forms the gradient Hardening wearing layer of the N-Si-C cross-linked network layer-inorganic carbide layer of ecto-entad; The degree of depth of described gradient Hardening wearing layer is 1 ~ 6um.
Preferably, described ion implanter is All directions ion implantation machine, produce the plasma body of multiple gases and solid element by radio frequency discharge and cathodic vacuum arc discharge, negative pulse high pressure can be applied on target platform, realize carrying out uniform surface ion injection to finished pieces with complex shapes.
Embodiment
In order to be illustrated more clearly in the present invention, below in conjunction with preferred embodiment, the present invention is described further.It will be appreciated by those skilled in the art that specifically described content is illustrative and nonrestrictive, should not limit the scope of the invention with this below.
Embodiment 1
Nylon 6 flat board after fully cleaning with second alcohol and water is put on ion implanter target platform, with 4 × 10
15ion/cm
2dosage inject argon plasma, form inorganic carbide layer on nylon 6 surface.Whole injection process keeps pressure in cavity to be 3 × 10
-2pa, target platform temperature is 80 DEG C.After injection completes, sample pressure in chamber is 3 × 10
-210min is kept under Pa.Then being again evacuated to pressure in chamber is 1 × 10
-3pa, with 6 × 10
15ion/cm
2dosage inject silicon plasma body, obtain the high firmly wear-resisting nylon 6 in surface dull and stereotyped.High firmly wear-resisting nylon 6 planar surface in described surface has gradient Hardening wearing layer, and this gradient Hardening wearing layer is the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.The degree of depth 1um of gradient Hardening wearing layer; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 0.5um.
Embodiment 2
Nylon66 fiber gear after fully cleaning with second alcohol and water is put on ion implanter target platform, with 5 × 10
17ion/cm
2dosage inject argon plasma, form inorganic carbide layer at nylon66 fiber gear surface.Whole injection process keeps pressure in cavity to be 1 × 10
-2pa, target platform temperature is 110 DEG C.After injection completes, sample pressure in chamber is 1 × 10
-230min is kept under Pa.Then being again evacuated to pressure in chamber is 1 × 10
-3pa, with 6 × 10
17ion/cm
2dosage inject silicon plasma body, obtain the high firmly wear-resisting nylon66 fiber gear in surface.The surface of the high firmly wear-resisting nylon66 fiber gear in described surface has gradient Hardening wearing layer, and this gradient Hardening wearing layer is the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.The degree of depth of gradient Hardening wearing layer is 6um; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 5um.
Embodiment 3
Nylon 12 pulley after fully cleaning with second alcohol and water is put on ion implanter target platform, with 5 × 10
17ion/cm
2dosage inject argon plasma, form inorganic carbide layer at nylon 12 pulley surface.Whole injection process keeps pressure in cavity to be 1 × 10
-2pa, target platform temperature is 100 DEG C.After injection completes, sample pressure in chamber is 1 × 10
-220min is kept under Pa.Then being again evacuated to pressure in chamber is 5 × 10
-3pa, with 6 × 10
16ion/cm
2dosage inject silicon plasma body, obtain high firmly wear-resisting nylon 12 pulley in surface.The surface of high firmly wear-resisting nylon 12 pulley in described surface has gradient Hardening wearing layer, and this gradient Hardening wearing layer is the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.The degree of depth of gradient Hardening wearing layer is 6um; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 5um.
Embodiment 4
Nylon 11 rod after fully cleaning with second alcohol and water is put on ion implanter target platform, with 1 × 10
16ion/cm
2dosage inject argon plasma, form inorganic carbide layer on nylon 11 rod surface.Whole injection process keeps pressure in cavity to be 3 × 10
-2pa, target platform temperature is 80 DEG C.After injection completes, sample pressure in chamber is 3 × 10
-210min is kept under Pa.Then being again evacuated to pressure in chamber is 5 × 10
-3pa, with 6 × 10
16ion/cm
2dosage inject silicon plasma body, form the gradient Hardening wearing layer of top-down Si-C cross-linked network layer-inorganic carbide layer on nylon 11 rod surface, obtain high hard wear resistant nylon 11 rod in surface.The degree of depth of the gradient Hardening wearing layer of the high firmly wear-resisting nylon 11 rod in described surface is 4um; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 1um.
Embodiment 5
The nylon66 fiber gear of the glass Hardening compound after fully cleaning with second alcohol and water is put on ion implanter target platform, with 1 × 10
16ion/cm
2dosage inject argon plasma, form inorganic carbide layer on its surface.Whole injection process keeps pressure in cavity to be 3 × 10
-2pa, target platform temperature is 90 DEG C.After injection completes, sample pressure in chamber is 3 × 10
-210min is kept under Pa.Then being again evacuated to pressure in chamber is 5 × 10
-3pa, with 6 × 10
16ion/cm
2dosage inject silicon plasma body, obtain high hard wear resistant nylon 66 gear in surface.The surface of the high firmly wear-resisting nylon66 fiber gear in described surface has gradient Hardening wearing layer, and this gradient Hardening wearing layer is the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.The degree of depth of gradient Hardening wearing layer is 5um; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 1um.
Embodiment 6
Nylon 12 after fully cleaning with second alcohol and water is put on ion implanter target platform, with 1 × 10
16ion/cm
2dosage inject argon plasma, form inorganic carbide layer on nylon 11 rod surface.Whole injection process keeps pressure in cavity to be 3 × 10
-2pa, target platform temperature is 80 DEG C.After injection completes, sample pressure in chamber is 3 × 10
-210min is kept under Pa.Then being again evacuated to pressure in chamber is 5 × 10
-3pa, with 6 × 10
16ion/cm
2dosage inject silicon plasma body.After injection completes, sample pressure in chamber is 3 × 10
-2keep 5min under Pa, be then evacuated to 2.6 × 10
-2pa, passes into High Purity Nitrogen, by 2 × 10
15ion/cm
2the nitrogen plasma of dosage is injected into nylon surface, obtains the high hard wear resistant nylon 12 in surface.The surface of the high firmly wear-resisting nylon 12 in described surface has gradient Hardening wearing layer, and this gradient Hardening wearing layer is the N-Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.The degree of depth of gradient Hardening wearing layer is 6um; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 1um.
Embodiment 7
Nylon 1010 roller after fully cleaning with second alcohol and water is put on ion implanter target platform, with 1 × 10
16ion/cm
2dosage inject argon plasma, form inorganic carbide layer on its surface.Whole injection process keeps pressure in cavity to be 3 × 10
-2pa, target platform temperature is 110 DEG C.After injection completes, sample pressure in chamber is 3 × 10
-210min is kept under Pa.Then being again evacuated to pressure in chamber is 1 × 10
-3pa, with 6 × 10
17ion/cm
2dosage inject silicon plasma body.After injection completes, sample pressure in chamber is 3 × 10
-2keep 5min under Pa, be then evacuated to 2.6 × 10
-2pa, passes into High Purity Nitrogen, by 6 × 10
17ion/cm
2the nitrogen plasma of dosage is injected into nylon 1010 roller surface, obtains the high hard wear resistant nylon nylon 1010 roller in surface.The surface of the high firmly wear-resisting nylon 1010 roller in described surface has gradient Hardening wearing layer, and this gradient Hardening wearing layer is the N-Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.The degree of depth of gradient Hardening wearing layer is 6um; Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%; The degree of depth of inorganic carbide layer is 1um.
Obviously; the above embodiment of the present invention is only for example of the present invention is clearly described; and be not the restriction to embodiments of the present invention; for those of ordinary skill in the field; can also make other changes in different forms on the basis of the above description; here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of extending out or variation be still in the row of protection scope of the present invention.
Claims (10)
1. the high hard wear resistant nylon in surface, is characterized in that: described nylon surface has gradient Hardening wearing layer; Described gradient Hardening wearing layer is the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad; The degree of depth of described gradient Hardening wearing layer is 1 ~ 6um; Carbon atom percentage composition in described inorganic carbide layer is not less than 95%; The degree of depth of described inorganic carbide layer is 0.5 ~ 5um.
2. the high hard wear resistant nylon in a kind of surface according to claim 1, is characterized in that: institute's gradient Hardening wearing layer is the N-Si-C cross-linked network layer-inorganic carbide layer of ecto-entad.
3. the high hard wear resistant nylon in a kind of surface according to claim 1, is characterized in that: described nylon be selected from the matrix material of nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and various nylon based one or more.
4. the preparation method of the high hard wear resistant nylon in a kind of surface as described in as arbitrary in claim 1-3, is characterized in that: adopt ion implanter to build the inorganic Hardening wearing layer of gradient at nylon surface in situ.
5. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 4, is characterized in that, comprise the steps:
1) nylon products ethanol and deionized water are cleaned up respectively rear naturally dry for subsequent use;
2) by step 1) in the nylon that obtains insert on ion implanter target platform, with 4 × 10
15~ 5 × 10
17ion/cm
2dosage inject argon plasma, form inorganic carbide layer on nylon surface; In whole injection process maintenance injection chamber, pressure is not higher than 3 × 10
-2pa, target platform temperature is 80 ~ 110 DEG C; After injection completes in chamber pressure not higher than 3 × 10
-210 ~ 30min is kept under Pa;
3) in ion implanter by step 2) in treated nylon in cavity pressure not higher than 5 × 10
-3under Pa, take HIGH-PURITY SILICON as negative electrode, with 6 × 10
15~ 6 × 10
17ion/cm
2dosage inject silicon plasma body, thus the high hard wear resistant nylon in obtained surface.
6. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 5, it is characterized in that: step 1) in, described nylon be selected from the matrix material of nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and various nylon based one or more.
7. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 5, is characterized in that: step 2) in, the carbon atom percentage composition in described inorganic carbide layer is not less than 95%; The degree of depth of described inorganic carbide layer is 0.5 ~ 5um.
8. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 5, it is characterized in that: step 3) in, the surface in situ of the high hard wear resistant nylon in obtained surface forms the gradient Hardening wearing layer of the Si-C cross-linked network layer-inorganic carbide layer of ecto-entad; The degree of depth of described gradient Hardening wearing layer is 1 ~ 6um.
9. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 5, is characterized in that: step 3) in, after silicon plasma body injects, also comprise and pass into High Purity Nitrogen again, in cavity, pressure is not higher than 3 × 10
-2under Pa, by 2 × 10
15~ 6 × 10
17ion/cm
2the nitrogen plasma of dosage injects nylon surface, thus the high hard wear resistant nylon in obtained surface; The surface in situ of the high hard wear resistant nylon in described surface forms the gradient Hardening wearing layer of the N-Si-C cross-linked network layer-inorganic carbide layer of ecto-entad; The degree of depth of described gradient Hardening wearing layer is 1 ~ 6um.
10. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 5, it is characterized in that: described ion implanter is All directions ion implantation machine, the plasma body of multiple gases and solid element is produced by radio frequency discharge and cathodic vacuum arc discharge, negative pulse high pressure can be applied on target platform, realize carrying out uniform surface ion injection to finished pieces with complex shapes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111909410A (en) * | 2020-07-27 | 2020-11-10 | 江苏博云塑业股份有限公司 | Composite nylon, preparation method thereof and spinning device |
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| CN103709742A (en) * | 2012-09-29 | 2014-04-09 | 黑龙江鑫达企业集团有限公司 | Modified aramid fiber reinforced PA66 material and preparation method thereof |
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| CN1224772A (en) * | 1998-01-24 | 1999-08-04 | 西南交通大学 | Synthesis of carbon-base film |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111909410A (en) * | 2020-07-27 | 2020-11-10 | 江苏博云塑业股份有限公司 | Composite nylon, preparation method thereof and spinning device |
| CN111909410B (en) * | 2020-07-27 | 2022-06-07 | 江苏博云塑业股份有限公司 | Composite nylon, preparation method thereof and spinning device |
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